Product derived from acid sludge and method of making the same



Jan. 5, 1926.

H. T. BENNETT ET Al.

PRODUCT DERIVED FROM ACID SLUDGE AND METHOD OF MAKING THE SAME Filed Dec. 20, 1924 2 Sheets-Sheet l Q Saai jtm.

Jan. 5 1926. Y 1,568,261

H. T. BENNETT ET AL y RODUCT DERIVED FROM ACID SLUDG AND METHOD OF MAKING THE SAME Filed Dec; 20, 1924 2 Sheets-Sheet 2 Patented' Jan. 5, 1.9.26.

UNITED STATES HARRY T. BENNETT, GEORGE f i A1,568,261 PATENT kiol-"FICE, i

MURPHY, AND Ln noY G. sToaY, or TULSA, OKLAHOMA.

PRODUCT DEBIVED FROM ACID SLUDGE AND METHOD OE M AK'ING THE SAME.

Appncatiun ined December 2o, 1924. serial No. 757,221.

To all whom z't may concern.'

Be it known that we, I-IARBY T. BENNETT,

rGEORGE B. MURPHY, and LE ROY G. STORY,

citizens of the United States ofV America 5 and residents of Tulsa, in the county of Tulsa, State of Oklahoma, have invented certain Products Derived fromAcid Sludge and Methods of Making the Same, of which the following is a full, clear, and exact description, reference being had to the accompanying drawings, forming a part of this specification.

This invention relates 'to products derived from acid sludge and methods of making the same, and more particularly to the treatment of the sludge obtained in the purification of petroleum products. It involves the addition of a solvent, which will be hereafter described, to the sludge. We have found by 205 actual experience that sludge, which has been regarded as an undesirable waste product, can be converted into a valuable product y -by merely commingling the solvent with the i sludge. .i Asphalt-like substances constitute some of the impurities of all petroleum products which for purification are usually treated with sulphuric acid, whereby the so-called acid-sludge is formed, and then with an absorbent or adsorbent material, such, for example, as fullers earth, as filtering and decolorizing agent. Whatever the urifying materials may be, they contain sai as haltlike substances, the recovery of whic together with other constituents of the acid sludge, is the object of our invention.

f To the accomplishment` of the foregoing and related eds the invention comprises the steps hereinafter fully described and more L0 particularly pointed' out in the appended claims. v

An approvedl method of carrying out our invention -is set forth in detail in the following description, but it is to be understood :5 that this specific disclosure does not set forth all of the several ways in which the principle of our invention may be used.

In the preferred form of our invention, the acid sludge containing asphalt-like impuri-ties is dissolved in a solvent and thereby converted into a solution adapted for use as a paint or impregnating solution, or for the manufacture of paving blocks, roofing material, and the like.

- products of an asphalt-base crude oil usually require a solvent containing a greater percentage of benzol.

The asphalt-like substances dissolved by and mixed with the solvent form the product resulting from one form of our improved process, but if desired, this solution may be distilled to remove and recover some or all of the solvent. The distillation of said solution to lseparate the solvent from the asphalt-likejsubstances may be carried out in any well known manner, by vaporizing the solvent and condensing its vapor, thus obtaining the original solvent as distillate, and the extracted asphalt-like substances as a residue or fbottom, which forms a useful product either as a lubricating stock, cracknkg product, fuel oil, paving material, or the 1 e.

According to the use of the product, the degree of distillation varies greatl For example, if the residue is to be use as impregnating fluid, it should contain considerable solvent, but if used as a paint, less sol-- vent is' required, whereas for paving, roofing or briquetting material practically no solvent should remain in the product. In the latter form, the product has the characteristic to set to a hard film, which, together with its cheapness of manufacture, makes it an appropriate base for pitch paints, Where it has the further advantage t at it 1s insoluble in acids and petroleum oils.

Fig. I is a diagrammatical view of an apparatus adapted for use in carrying out our method.

Fig. II is a view similar to Fig. I illustrating another form of the invention.

The apparatus shown by Fig. I comprises an ordinary acid agitator 1 provided with an intake" ipe 2, and a discharge pipe 3 for the treate oil. The acid sludge is removed through a pipe 4 leading to a mixing tank 5. y

Water may be admitted/ tothe tank by means of pipe 6 and discharged through sist of alcohol 30 percent pipe 7. To remove the solution from tank 5, a pipe 8 is provided with a pump 9 and a branch-10. The pipe 8 leads to a still 11 equipped With a condenser 12 and a residuiim outlet 13.

In carrying out the" product, such as a residuum from which gasoline and kerosene have .been removed. may be transmitted to the acid agitator and theretreated `With'sulphuric acid in the usual manner. The treated oil is removed through pipe 3 and the acid sludge is conducted through pipe 4 to the mixing tank 5, .Where it is coinmingled with a solvent which preferably comprises denatured alcohol and a-coal tar product such as benzol. We have found that both of these fluids are desirable in the' solvent, because each will dissolve some products that would not be dissolved by the other, and the mixture of alcohol and benzol will dissolve substances that would not be dissolved by successive treatments with alcohol and benzol. Consequently, the solvent produced by mixing these fluids is an important factor the preferred form of our process, although the invention comprehends modifications and equivalents within Ithe scope of the claims hereunto appended.

To be more specific, the solvent may conand benzol percent. This Vsolvent is coinmingled with the sludge in tank 5, and Without any further treatment the resultant mixture may be withdrawn through pipe 10 and used as apaint, although it is desirable tocadd a small quantity of linseed oil, or the like. .A satisfactory paint can be composed of acid sludge 20 percent, solvent 7 5 percent and linseed oil 5 percent. The paint produced in this simple manner is a heat-resisting roduct ladapted for use en smoke stacks and other articles exposed to high temperatures. y

In makingsome other products it is desirable'to remove a part or all of the solvent, and in some cases it is desirable to employ an excess of the solvent so as to reduce the viscosity of the sludge. In these instances, the solution may be transmitted through pipe 8 to the still 11 and distilled .to recover the solvent from condenser 12,

the asphaltio product. being discharged through pipe 13 as a residuum.

Water ma be introduced through pipe 6 to wash yacid from the mixture in tan 5, and in this .event the acid-containing water is removed through pipe 7..

In the system,shown by.Fig. Il, an acid agitator 15 is provided with an intake pipe 16 for the admission of gasoline, kerosene,

lubricating oil, or other oil containing'impurities. The treated oil is` discharged process, a petroleum through a' pipe 17 and the acid sludge is conducted through pipe 18 to a mixing tank 419 Where it is Washed and then permitted to settle. Steam may be introduced through pipe 2Q. The stratification results in the separation of acid oil and Weak acid from the sludge, as suggested by the drawing. The tank 19 Vis provided With a discharge pipe 21 for the Weak acid, a pipe 22 for the i discharge of acid oil, and a pipe 23 .through which acid sludge is conducted to a mixing tank 24, each of said pipes being provided with a valve as shown in the drawing.

The sludge in tank 24 is mixed with a solvent such as alcohol and benzol and the resultant solution is Withdrawn through discharge pipe 25.

treatment of a petroleum product With sulphuric acid.

4. The method of converting acid sludge of the character described into useful roduets which comprises Washing the s udge with Water and coinmingling ithe sludge with a solvent comprising a coal tar product and alcohol.

5.l '.lhe method of converting acid sludge containing asphalt-like substances into usefu l products, which comprises commingling a solvent including alcohol and a coal tariproduct with the acidA sludge, and distilling the resultant solution to remove the excess solvent therefrom.

6. lhe method of converting acid lsludge containing asphalt-like substances into useful products, which comprises mixing and digesting said sludge with Water and a solvent comprisin alcohol and a coal tar product, thereby dissolvingits ac id content in the Water and the asphalt-like substances in said solvent,`and separating the acid-containing Water from the dissolved asphaltlike substances.

7. A new article of manufacture comprising acid sludge residue dissolved in a solveit including alcohol and a coal tar produc E As a new article of manufacture, a paint comprising acid slude residue dissolved in a solvent benzol.

including alcohol and 9. As a new article ofma-nufacture, ai

l mixture containing acid sludge residue with` asphalt-like substances therem, and a v'exellvent including alcohol' and a coal tar product. y

' 1l. As e` new article ofV manufacturera I mixture containingacid slude residuewith `asphalt-like substances therein, and a.

of the mixture and the solvent being lessy than 5 A In testimony-that weclaimthe foregoingl ereent.

We hereunto aix our s1 atures.l

i l HARRY T; BENNETT. GEORGE vB. VMURPHY. LE ROY G.STORY. 

